Separation and purification method for Thonningianin A monomer

A separation and purification, monomer technology, applied in the field of separation and purification of traditional Chinese medicine, to achieve the effect of short production cycle, low solvent consumption and high academic value

Active Publication Date: 2014-03-26
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no relevant report on the isolation of high-purity Thonningianin A monomer product from C.

Method used

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  • Separation and purification method for Thonningianin A monomer
  • Separation and purification method for Thonningianin A monomer
  • Separation and purification method for Thonningianin A monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] (1) extract

[0053] Take 1 kg of Herba japonica and cut it into 0.5 cm segments, add 6 L of 70% ethanol solution, reflux extraction 3 times, 2 hours each time, filter, collect and combine the filtrates;

[0054] (2) concentrated

[0055] Recover ethanol from the collected and combined filtrate in step (1), and concentrate to a volume of 3.5L;

[0056] (3) Macroporous adsorption resin enrichment and elution

[0057] Pass the concentrated filtrate of step (2) through a macroporous adsorption resin chromatography column with a diameter of 10 cm for adsorption, first wash the resin with purified water until it is colorless, and then elute the product with 60% ethanol until the effluent Colorless, collect and combine the eluents for a total of 5 L, concentrate the eluents under reduced pressure, recover ethanol, and obtain 1.5 L of concentrated solutions;

[0058] (4) Polyamide resin enrichment and elution

[0059] Pass the concentrated solution obtained in step (3) thr...

Embodiment 2

[0073] (1) extract

[0074] Take 10 kilograms of the herba japonica medicinal material and cut it into 0.5 cm sections, add 60 L of 70% ethanol solution, reflux extraction for 3 times, each time for 2 hours, filter, collect and combine the filtrates;

[0075] (2) concentrated

[0076] Recover the ethanol from the collected and combined filtrate in step (1), and concentrate to a volume of 35 L.

[0077] (3) Macroporous adsorption resin enrichment and elution

[0078] Pass the concentrated filtrate of step (2) through a macroporous adsorption resin chromatography column with a diameter of 10 cm for adsorption, first wash the resin with purified water until it is colorless, and then elute the product with 70% ethanol until the effluent Colorless, collect and combine the eluents for a total of 5 L, concentrate the eluents under reduced pressure, recover ethanol, and obtain 14 L of concentrated solutions;

[0079] (4) Polyamide resin enrichment and elution

[0080] Pass the con...

Embodiment 3

[0094] (1) extract

[0095] Take 50 kilograms of Herba japonica medicinal materials and cut them into 0.5 cm segments, add 300 L of 70% ethanol solution, reflux extraction 3 times, each time for 2 hours, filter, collect and combine the filtrates;

[0096] (2) concentrated

[0097] The ethanol was recovered from the collected and combined filtrate in step (1), and concentrated to a volume of 180L.

[0098] (3) Macroporous adsorption resin enrichment and elution

[0099] Pass the concentrated filtrate of step (2) through a macroporous adsorption resin chromatography column with a diameter of 25 cm for adsorption, first wash the resin with purified water until it is colorless, and then elute with 65% ethanol until the effluent has no Color, collect and combine eluent 220L altogether, eluate is concentrated under reduced pressure, reclaims ethanol, obtains concentrated solution 14L;

[0100] (4) Polyamide resin enrichment and elution

[0101] Pass the concentrated solution obt...

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Abstract

The invention relates to a separation and purification method for a Thonningianin A monomer and belongs to the technical field of separation and purification of active components of traditional Chinese medicines. The separation and purification method comprises the specific steps of (1) extraction: cutting penthorum chinense pursh into small pieces, performing backflow extraction on the small pieces through ethanol, and then filtering the small pieces; (2) concentration: concentrating filtrate to 20 percent; (3) enrichment and elution of macroporous adsorption resin; (4) enrichment and elution of polyamide resin; (5) high-efficiency preparation and liquid chromatographic separation, wherein the flowing phase is an acetonitrile-3% phosphoric acid aqueous solution, and the detection wavelength is 254nm; (6) product recycling: filtering a Thonningianin A monomer solution to separate out crystals, and drying the crystals to obtain the Thonningianin A monomer product. The separation and purification method is easy and convenient to operate, short in production period, high in separation efficiency, stable and reliable in technology and high in reproducibility; the cost is easy to control, and the product is high in purity; the Thonningianin A monomer can be used as a standard substance for measuring the content.

Description

technical field [0001] The invention relates to a method for separating and purifying medicinal plant compound monomers, in particular to a method for separating and purifying Thonningianin A monomers from Herba japonica, belonging to the technical field of separation and purification of traditional Chinese medicines. Background technique [0002] Penthorum chinense Pursh is the dry aerial part of the plant Penthorum chinense Pursh in the family Saxifragaceae. Collected in summer and autumn, remove impurities, dry or use fresh. Crimson yellow grass is a traditional medicine of the Miao nationality, and the whole herb is used as medicine by the people. The whole herb is warm in nature, sweet in taste, non-toxic, and has the functions of clearing heat, diuresis, detoxification, promoting blood circulation, calming the liver, strengthening the spleen, and dispelling jaundice. Indications for jaundice, edema, amenorrhea, metrorrhagia, leukorrhagia, bruises, and various types o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H1/08
CPCY02P20/582
Inventor 白兰辉文焕松夏柯郭建华刘丁
Owner CHENGDU PUSH BIOLOGICAL TECH
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